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University of Oklahoma A.B.

Cerato

Procedure for EGME Surface Area Determination


University of Oklahoma A.B. Cerato

STEP 1:

Desiccant

1. Weigh 120 grams of CaCl2 into a 1-L beaker and dry in oven for 1 hour
2. Weigh 20 grams of EGME into a 400 mL beaker
3. Remove CaCl2 from oven and weigh out 100 grams without cooling
4. Add to the beaker containing EGME and mix immediately
5. After solvate has cooled, place in a culture chamber and spread uniformly over
bottom
6. Store the culture chamber in sealed desiccator.

STEP 2:

Preparing the sample

1. Place approximately 1 gram of oven dried soil passing a #40 sieve in the bottom of a
clean dry aluminum or glass tare having dimensions of approximately 76 mm in
diameter by 20 mm in height.
2. Determine the mass of the soil to the nearest 0.001 g.
3. Using a small pipette, gently place approximately 3 mL of laboratory grade EGME
over the soil.
4. Gently mix the soil and EGME together using a slow swirling motion of the hand until
the mixture forms a slurry and the appearance of the slurry is uniform. It is important
not to place a stirrer in the mixture, as any loss of soil would directly affect the surface
area measurement. Swirling the mixture in the aluminum tare with a circular hand
motion allows for no soil loss and a uniform coverage of all soil particles by the
EGME.
5. Place the tare into a vacuum desiccator and place a small plexiglass lid over the tare,
leaving a gap of 2 to 3 mm between the lid and the tare.
6. Attach the lid of the desiccator to a vacuum pump and begin evacuating using a
vacuum of at least 635 mm Hg.
7. After 12 to 16 hours, remove the tare and determine the mass of the soil/EGME
mixture. Repeat this step again at approximately 24 hours. The weight of the mixture
should not vary more than 0.001 g. If the weight varies by more than 0.001 g, place
the tare back in the desiccator and weigh it again in approximately 4 hours.

STEP 3:

Calculating SSA

Calculate SSA as
Wa
SSA =
0.000286Ws
University of Oklahoma A.B. Cerato

where:

SSA = Specific Surface Area in m2/g


Wa = weight of ethylene glycol monoethyl ether (EGME) retained by the sample
in grams (final slurry weight Ws)
0.000286 = weight of EGME required to form a monomolecular layer on a square
meter of surface (g/m2)
Ws = oven dry weight of soil (g)

It is recommended that periodically a control sample be tested to monitor the accuracy


of the tests.

Example:

Initial Tin Weight: 30.0485 g


Initial Soil Weight (Ws): 1.0030 g
18 hour tare + slurry weight: 31.0634 g
18 hour slurry weight: 31.0634 30.0485 = 1.0149 g
24 hour tare + slurry weight: 31.0625 g
24 hour slurry weight: 31.0625-30.0485 = 1.014 g
Wa = 1.014 1.0030 =0.011 g
SSA = 0.011 g/(1.0030 g* 0.000286) = 38 m2/g

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